EP2692471B1 - Tool for friction stir processing and method for friction stir processing using same - Google Patents

Tool for friction stir processing and method for friction stir processing using same Download PDF

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Publication number
EP2692471B1
EP2692471B1 EP12763193.5A EP12763193A EP2692471B1 EP 2692471 B1 EP2692471 B1 EP 2692471B1 EP 12763193 A EP12763193 A EP 12763193A EP 2692471 B1 EP2692471 B1 EP 2692471B1
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EP
European Patent Office
Prior art keywords
phase
friction stir
tool
heat treatment
intermetallic compound
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EP12763193.5A
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German (de)
English (en)
French (fr)
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EP2692471A4 (en
EP2692471A1 (en
Inventor
Takayuki Takasugi
Yasuyuki Kaneno
Sachio Oki
Tomotake Hirata
Noboru Mochizuki
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Kinki University
Osaka Prefecture University PUC
ISEL Co Ltd
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Kinki University
Osaka Prefecture University PUC
ISEL Co Ltd
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Publication of EP2692471A4 publication Critical patent/EP2692471A4/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
    • B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
    • B23K20/1245—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding characterised by the apparatus
    • B23K20/125—Rotary tool drive mechanism
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
    • B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
    • B23K20/1245—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding characterised by the apparatus
    • B23K20/1255—Tools therefor, e.g. characterised by the shape of the probe
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

Definitions

  • the present invention relates to a friction stir processing tool which is capable of subjecting a work of a metal material such as iron or an iron alloy to friction stir processing over a long period of time, and a method for friction stir processing using the friction stir processing tool.
  • the maximum ultimate temperature does not reach a melting point and joining is performed in a solid phase state because joining is performed utilizing frictional heat between a tool and a work. Therefore, there is the advantage that as compared to melt-welding such as arc welding, a decrease in strength of a joint is small, joining defects such as voids and cracks do not occur, the joint surface is flat, and so on.
  • friction stir processing FSP
  • FSP friction stir processing
  • FSJ friction spot joining
  • a tool made of steel such as SKD steel is used for a tool when aluminum or an aluminum alloy is used as a work in the friction stir processing.
  • the tool made of steel such as SKD steel has the problem that it is soon deformed due to attrition or the like, so that joining cannot be performed.
  • a tool made of ceramic has the problem that it is expensive and is easily broken, and it is easily worn away particularly when the work is stainless steel. If very small pieces of a material of a tool made of ceramic are dispersed in an iron-based work, for example stainless steel when the tool is worn away due to friction stir processing, mechanical properties and corrosion resistance may be degraded.
  • Ni-based dual multi-phase intermetallic compound alloy which is a material of this tool includes a Ni 3 Al-Ni 3 Nb-Ni 3 V-based intermetallic compound alloy or a Ni 3 Al-Ni 3 Ti-Ni 3 V-based intermetallic compound alloy.
  • the Ni-based dual multi-phase intermetallic compound alloy is a multi-phase alloy formed by combining Ni 3 X type intermetallic compounds, and has excellent hardness as compared to an alloy formed of a single intermetallic compound phase.
  • a friction stir processing tool made of a Ni-based dual multi-phase intermetallic compound alloy is particularly suitable for friction stir processing of a work of iron, an iron alloy or the like which requires a high processing temperature because necessary hardness is maintained even when the temperature is increased (to 800°C or higher) by frictional heat during processing to the extent that the tool side face emits light in orange color.
  • Patent Document 1 Japanese Patent Laid-open Publication No. 2009-255170
  • the aforementioned friction stir processing tool including a Ni-based dual multi-phase intermetallic compound alloy shows high hardness even at a high temperature, but when the tool is continuously used over a long period of time and resultantly tool abrasion proceeds, friction stir processing can no longer be properly performed with the tool, and no further use is possible. Accordingly, in the friction stir processing tool including a Ni-based dual multi-phase intermetallic compound alloy, it is desired to achieve further improvement of its properties, i.e. further high hardness, so that even when the tool is continuously used at a high temperature, tool abrasion can be kept low to increase a tool life.
  • the present invention has been devised in view of the above situations, and an object thereof is to provide a friction stir processing tool including a Ni-based dual multi-phase intermetallic compound alloy, wherein by exhibiting further excellent hardness even at a high temperature, tool abrasion is kept low to increase a tool life, and a method for friction stir processing using the tool.
  • a Ni-based dual multi-phase intermetallic compound alloy as a material of a friction stir processing tool has contained an element (e.g. Ta, Nb, Ti, etc.) to replace the X element of a Ni 3 X type intermetallic compound, but the present inventors have come up with the idea to include an element to replace the Ni element rather than the X element of the Ni 3 X type intermetallic compound, thus making it possible to achieve the aforementioned object.
  • an element e.g. Ta, Nb, Ti, etc.
  • a friction stir processing tool includes a Ni-based dual multi-phase intermetallic compound alloy containing Re.
  • the Ni-based dual multi-phase intermetallic compound alloy contains 10 to 1000 ppm by weight of B based on the total weight of 100 atom% in total of a composition including Ni as a main component and 5 to 12 atom% of Al, 11 to 17 atom% of V and 1 to 5 atom% of Re, and has a dual multi-phase constitution of a proeutectoid L1 2 phase and a (L1 2 +D0 22 ) eutectoid constitution.
  • the Ni-based dual multi-phase intermetallic compound alloy preferably has a composition including 10 to 1000 ppm by weight of B based on the total weight of 100 atom% in total of a composition including Ni as a main component and 8 to 12 atom% of Al, 13 to 17 atom% of V and 1 to 5 atom% of Re, or a composition including 10 to 1000 ppm by weight of B based on the total weight of 100 atom% in total of a composition including Ni as a main component and 5 to 9 atom% of Al, 11 to 15 atom% of V, 3 to 7 atom% of Ta and 1 to 5 atom% of Re.
  • the Ni-based dual multi-phase intermetallic compound alloy is formed by casting, while gradually cooling, a melt containing all the components of the composition.
  • the Ni-based dual multi-phase intermetallic compound alloy is preferably formed by performing a heat treatment (heat treatment at 1230 to 1330°C or/and 800 to 1000°C) after casting.
  • a method for friction stir processing wherein a work is softened by frictional heat generated when the friction stir processing tool, while rotating, is pressed against the work to be processed.
  • a friction stir processing tool includes a Ni-based dual multi-phase intermetallic compound alloy, and therefore further high hardness is exhibited to improve abrasion resistance, so that even a long period of friction stir processing can be endured.
  • High hardness can be reliably exhibited by heat-treating the alloy material. Therefore, even a work of iron, an iron alloy or the like which requires a high processing temperature can be subjected to friction stir processing properly over a long period of time.
  • a friction stir processing tool (hereinafter, referred to a "tool" as appropriate) of this embodiment is a tool for softening a work of a metal material by frictional heat generated when the tool, while rotating, is pressed against the work to be processed.
  • This tool is used for friction stir processing in general including friction stir welding (FSW), friction stir processing (FSP) and friction spot joining (FSJ) which have been described in Background Art.
  • FSW friction stir welding
  • FSP friction stir processing
  • FSJ friction spot joining
  • a friction stir processing tool 1 has a columnar shoulder portion 11, and a columnar attaching portion 13 having a diameter larger than that of the shoulder portion 11 and having a cut surface 12 formed on the side face.
  • the attaching portion 13 of the friction stir processing tool 1 is put into a tool holder or the like of a friction stir processing apparatus, and tightened with a bolt abutted against the cut surface 12 of the attaching portion 13, so that the friction stir processing tool 1 is detachably attached.
  • the end face of the shoulder portion 11 has a planar shoulder surface 2 and a spherical probe 3 projectingly provided at the central part of the shoulder face 2.
  • the tool 1 presses the shoulder surface 2 and the probe 3 against the work while rotating to generate frictional heat.
  • the shape of the tool 1 is limited to that in Fig. 1 , and may be a shape with a flange formed between the shoulder portion 11 and the attaching portion 13, or the attaching portion 13 may be in a polygonal shape.
  • the shoulder surface 2 is not limited to a planar shape, and may be formed in a slightly convex or slightly concave shape with the probe 3 situated at the center.
  • the probe 3 is not limited to a spherical shape, and may be in a columnar shape or a truncated cone shape, or may be screwed.
  • the shoulder diameter (diameter of shoulder surface 2) is set to about 8 to 14 mm in the case of a work having a plate thickness of 1. 5 mm or less.
  • the probe diameter (diameter of the thickest portion of probe 3) is set to about 3 to 6 mm, and the length of the probe 3 (projecting height from shoulder surface 2), depending on the plate thickness of a work, is set to a such length that the probe 3 is deeply inserted into the work but its tip does not pass through the work to project therefrom.
  • the length of the probe 3 is set to a length smaller than the thickness of the work by about 0.1 to 0.2 mm.
  • the tool 1 is used by being attached to a known friction stir welding apparatus including machine three shafts : a platen shaft (X), a traverse shaft (Y) and a lifting shaft (Z).
  • a known friction stir welding apparatus including machine three shafts: a platen shaft (X), a traverse shaft (Y) and a lifting shaft (Z).
  • the tool 1 is used by being attached to a known five shaft frame type friction stir welding apparatus including machine three shafts: a platen shaft (X), a traverse shaft (Y) and a lifting shaft (Z) and tool two shafts: a rocking shaft and a pivot shaft.
  • the tool 1 is also used by being attached to a machine head mounted at the tip of a known robot arm including three joint shafts and two rotary shafts.
  • friction stir welding is performed in the following manner.
  • the backing material 5 is used for preventing contamination or the like from the back surface by friction stir welding, and preferably has heat resistance, nonflammability, strength, contamination resistance, surface smoothness and the like, and a plate, a molded product, a foil or the like, which is formed of a material such as a high-melting point metal, ceramic or
  • silicon nitride silicon nitride
  • the probe 3 of the friction stir processing tool 1 while rotating at a high speed, is press-fitted to one end of the butting portion 7 of the plate-shaped bodies 6a and 6b, and pressed so that the shoulder surface 2 of the tool 1 comes into contact with the surfaces of the plate-shaped bodies 6a and 6b (70% in terms of a contact surface). Consequently, by friction between the probe 3 rotating at a high speed and the shoulder surface 2, the vicinity of the butting portion 7 of the plate-shaped bodies 6a and 6b is heated to be softened.
  • the rotating friction stir processing 1 is moved toward the other end side along the butting portion 7 of the plate-shaped bodies 6a and 6b. Consequently, a portion including the butting portion 7 of the plate-shaped bodies 6a and 6b is softened by continuously generating heat by friction, and stirred so that the butting portion 7 of the plate-shaped bodies 6a and 6b are frictionally joined.
  • the forwarding speed of the tool 1 is preferably set to 900 to 1400 mm/min for processing iron or an iron alloy as a work with high quality.
  • the rotation number of the tool 1 is preferably such a rotation number that when the tool 1 is brought into press-contact with a work of iron or an iron alloy, the work is heated to about 800°C to about 1000°C by frictional heat.
  • the rotation number is preferably set to 600 to 900 rpm.
  • the lead angle of the tool 1 (inclination to the vertical line when the tip portion of the tool is inclined to the traveling direction side) is preferably set to 2 to 5°.
  • the material of the friction stir processing tool 1 includes a Ni-based dual multi-phase intermetallic compound alloy containing rhenium(Re).
  • the Ni-based dual multi-phase intermetallic compound alloy includes Ni, V, Al, Ta (Ta is an optional component), B and Re (including unavoidable impurities) and has a dual multi-phase constitution of a proeutectoid L1 2 phase and a (L1 2 +D0 22 ) eutectoid constitution.
  • Fig. 3 shows the constitution of the Ni-based dual multi-phase intermetallic compound alloy: Fig. 3A shows a SEM photograph (left side) and a TEM photograph (right side) of the constitution; and Fig. 3B is a schematic view of the constitution.
  • Fig. 4 shows a schematic view of a crystal structure of a phase which forms the constitution of the Ni-based dual multi-phase intermetallic compound alloy: Fig. 4A shows a Ni 3 Al (L1 2 ) phase; and Fig. 4B shows a Ni 3 V(D0 22 ) phase.
  • the constitution of the Ni-based dual multi-phase intermetallic compound alloy includes a cuboid microstructures formed with good consistency, and nanostructures formed between the microstructures.
  • the former microstructure includes a cuboid proeutectoid L1 2 phase (Ni 3 Al) and a channel portion which is a gap thereof.
  • the latter nanostructure is formed in the channel portion, and includes a eutectoid constitution formed of a L1 2 phase and a D0 22 phase (Ni 3 Al and Ni 3 V).
  • an upper multi-phase constitution with a proeutectoid L1 2 phase precipitated in an A1 phase is formed by a heat treatment at a temperature higher than an eutectoid temperature, and by a subsequent heat treatment at a temperature equal to or lower than the eutectoid temperature, the A1 phase is eutectoid-transformed (decomposed) into two phases: a L1 2 phase and a D0 22 phase to form a lower multi-phase constitution.
  • the temperature higher than an eutectoid temperature is a temperature at which the proeutectoid L1 2 phase and the A1 phase coexist, and the eutectoid temperature is an upper limit value of the temperature at which the A1 phase is transformed (decomposed) into a L1 2 phase and a D0 22 phase.
  • the Ni-based dual multi-phase intermetallic compound alloy is formed by diploidizing a Ni 3 X type intermetallic compound showing excellent properties.
  • Re rhenium
  • Re rhenium
  • Re is included as an element to replace the Ni element of the Ni 3 X type intermetallic compound in the Ni-based dual multi-phase intermetallic compound alloy. That is, by including Re in a Ni-based dual multi-phase intermetallic compound alloy containing Ni, Al and V, a Ni-based dual multi-phase intermetallic compound alloy having fine dual multi-phase constitutions is obtained, and the hardness of the alloy is improved. Further, by including Re in a Ni-based dual multi-phase intermetallic compound alloy containing Ta in addition to Ni, Al and V, the hardness of the alloy is further improved. B is added for enhancing the ductility of the obtained alloy by suppressing intergranular cracking.
  • the hardness of the alloy can be further improved while the dual multi-phase constitution is maintained. Accordingly, the alloy material before heat treatment is easily processed (e.g. cutting processing) into a tool shape, and hardness can be improved after the material is processed into a tool shape. Therefore, the friction stir processing tool 1 having excellent processability (e.g. cutting processability) and high hardness is obtained using the Ni-based dual multi-phase intermetallic compound alloy containing Re.
  • the Ni-based dual multi-phase intermetallic compound alloy can be produced by the following production method.
  • an upper multi-phase constitution including a proeutectoid L1 2 phase and an A1 phase is formed, and further the A1 phase is decomposed to form a lower multi-phase including a L1 2 phase and a D0 22 phase.
  • the gradual cooling is performed by, for example, furnace cooling. That is, the materials are heated to be melted and after heating, the melt is left standing in the furnace.
  • the Ni-based dual multi-phase intermetallic compound alloy having the aforementioned constitutions is preferably heat-treated after casting.
  • a homogenization heat treatment a solution heat treatment, an aging heat treatment, a first heat treatment, a second heat treatment and the like are shown as an example.
  • a solution heat treatment (solution heat treatment for A1 haploidization) is performed.
  • the solution heat treatment is performed at 1230 to 1330°C. Specifically, it is preferred to perform a heat treatment at a temperature of 1280°C for about 5 hours.
  • a homogenization heat treatment may be performed as another step before the solution heat treatment, or the solution heat treatment may also serve as a homogenization heat treatment.
  • Cooling is performed after the solution heat treatment, and the cooling may be either natural cooling such as air cooling or forced cooling such as water cooling, and may be, for example, cooling by furnace cooling.
  • the V element or the like is solid-dissolved in Ni to form an A1 phase (Ni solid solution phase), a L1 2 phase is precipitated in the A1 phase by subsequent cooling, and further the A1 phase is decomposed into a L1 2 phase and a D0 22 phase, so that a dual multi-phase constitution (constitution of proeutectoid L1 2 phase and (L1 2 +D0 22 ) eutectoid constitution) is formed again. Accordingly, a Ni-based dual multi-phase intermetallic compound alloy including fine and uniform dual multi-phase constitutions is provided.
  • An alloy material (ingot, etc.) obtained by melting/solidification may be subjected to a first heat treatment at a temperature at which the proeutectoid L1 2 phase and the A1 phase coexist (formation of upper multi-phase constitution), and thereafter cooled to a temperature at which the L1 2 phase and the D0 22 phase coexist (natural cooling such as air cooling or furnace cooling, or forced cooling such as water cooling), or subjected to a second heat treatment at a temperature at which the L1 2 phase and the D0 22 phase coexist, thereby changing the A1 phase into a (L1 2 +D0 22 ) eutectoid constitution (formation of lower multi-phase constitution).
  • the first heat treatment is performed at a temperature of, for example, 1230 to 1330°C, and specifically the heat treatment is performed at a temperature of 1280°C for about 5 to 200 hours.
  • the second heat treatment is performed at a temperature of, for example, 800 to 1000°C, and specifically the heat treatment is performed at a temperature of 930°C for 5 to 200 hours.
  • the solution heat treatment may also serve as the first heat treatment.
  • the aging heat treatment is performed for forming a L1 2 phase and a D0 22 phase by transforming (decomposing) an A1 phase formed in a gap of proeutectoid L1 2 phases in a Ni-based dual multi-phase intermetallic compound alloy, and therefore can be performed by carrying out a heat treatment in the same temperature range as in the second heat treatment. That is, preferably the aging heat treatment is at a temperature of 800 to 1000°C, preferably 825 to 1000°C (850 ⁇ 25°C or 975 ⁇ 25°C) for about 0.5 to 24 hours for accelerating formation of a L1 2 phase and a D0 22 phase.
  • the aging heat treatment may be performed after casting, or performed after the first or (and) second heat treatment.
  • the aging heat treatment is also referred to as a lower multi-phase heat treatment (heat treatment for forming a lower multi-phase constitution).
  • Ni-based dual multi-phase intermetallic compound containing Re which forms the friction stir processing tool 1
  • examples of the Ni-based dual multi-phase intermetallic compound containing Re, which forms the friction stir processing tool 1 include those that contain 10 to 1000 ppm by weight of B based on the total weight of 100 atom% in total of a composition including Ni as a main component and 5 to 12 atom% of Al, 11 to 17 atom% of V and 1 to 5 atom% of Re, and have a dual multi-phase constitution of a proeutectoid L1 2 phase and a (L1 2 +D0 22 ) eutectoid constitution.
  • Ni-based dual multi-phase intermetallic compound alloy examples include those that have a composition including 10 to 1000 ppm by weight of B based on the total weight of 100 atom% in total of a composition including Ni as a main component and 8 to 12 atom% of Al, 13 to 17 atom% of V and 1 to 5 atom% of Re, and unavoidable impurities, and have a dual multi-phase constitution of a proeutectoid L1 2 phase and a (L1 2 +D0 22 ) eutectoid constitution.
  • the Ni-based dual multi-phase intermetallic compound alloy containing Re exhibits significantly high hardness due to formation of fine dual multi-phase constitutions, and therefore the friction stir processing tool 1 including the Ni-based dual multi-phase intermetallic compound alloy can be significantly improved in hardness.
  • the Ni-based dual multi-phase intermetallic compound of the aforementioned composition is further significantly improved in hardness when subjected to an aging heat treatment (e.g. heat treatment at 800 to 1000°C) after the solution heat treatment. Since the Ni-based dual multi-phase intermetallic compound alloy shows significantly high hardness at the temperature of the aforementioned heat treatment, the friction stir processing tool 1 which is also suitable for use at a high temperature (e.g. temperature of the aforementioned aging heat treatment) is obtained.
  • Ni-based dual multi-phase intermetallic compound alloy containing Re can exhibit a Vickers hardness of more than about 660 HV when subjected to an aging heat treatment, for example, at 900°C for 5 to 10 hours (see sample No. 1 in Table 2 described later).
  • the Ni-based dual multi-phase intermetallic compound alloy containing Re, which forms the friction stir processing tool, may further contain Ta.
  • the Ni-based dual multi-phase intermetallic compound alloy in this case include those that have a composition including 10 to 1000 ppm by weight of B based on the total weight of 100 atom% in total of a composition including Ni as a main component and 5 to 9 atom% of Al, 11 to 15 atom% of V, 3 to 7 atom% of Ta and 1 to 5 atom% of Re, and unavoidable impurities, and have a dual multi-phase constitution of a proeutectoid L1 2 phase and a (L1 2 +D0 22 ) eutectoid constitution.
  • the Ni-based dual multi-phase intermetallic compound of the aforementioned composition which contains Ta and Re, not only can be significantly improved in hardness when subjected to an aging heat treatment (e.g. heat treatment at 800 to 1000°C) after a solution heat treatment, but also has excellent hardness after the solution heat treatment and before the aging heat treatment, and therefore the friction stir processing tool 1 including the Ni-based dual multi-phase intermetallic compound alloy containing Ta and Re can be significantly improved in hardness. Since the Ni-based dual multi-phase intermetallic compound alloy can also be significantly improved in hardness by the heat treatment while maintaining fine dual multi-phase constitutions, the friction stir processing tool 1 which is also suitable for use at a high temperature (e.g. temperature of the aforementioned aging heat treatment) is obtained.
  • a high temperature e.g. temperature of the aforementioned aging heat treatment
  • Ni-based dual multi-phase intermetallic compound alloy containing Ta and Re can exhibit a Vickers hardness of more than about 780 HV when subjected to an aging heat treatment, for example, at 900 to 950°C for 2 to 24 hours (see sample No. 2 in Tables 2 and 3 described later).
  • the Ni-based dual multi-phase intermetallic compound which forms the friction stir processing tool 1 is significantly improved in hardness while forming fine dual multi-phase constitutions when Re is added. Accordingly, in the friction stir processing tool 1, further excellent hardness is exhibited even at a high temperature during friction stir processing, so that tool abrasion by friction stir processing is kept low to increase a tool life. Therefore, even for a work of iron, an iron alloy or the like which requires a high processing temperature, the tool 1 can ensure a long period of friction stir processing, and friction stir processing can be performed with high quality over a long period of time. Further, since the tool replacement frequency is low, processing costs can be reduced.
  • the iron alloy as used herein refers to an alloy containing iron as a main component and one or more other elements. Examples thereof include carbon steel and stainless steel.
  • base metals of Ni, Al, V, Ta and Re in the ratio shown in Table 1 each having a purity of 99.9% by weight
  • B base metals of Ni, Al, V, Ta and Re in the ratio shown in Table 1 (each having a purity of 99.9% by weight) and B were melted and solidified in a mold within an arc melting furnace to prepare a cast material (button-shaped alloy of 30 to 50 mm ⁇ ).
  • test pieces (about 10mm x 5mm x 1mm) were cut out from the prepared cast material, and the obtained test pieces were subjected to a heat treatment at 1280°C for 5 hours as a solution heat treatment, followed by performing furnace cooling.
  • test pieces subjected to the solution heat treatment were heat-treated at a temperature of 900°C for 5, 10 and 24 hours and at a temperature of 950°C for 2, 5, 10 and 24 hours, respectively, as a lower multi-phase heat treatment (aging treatment), and water quenching was performed.
  • aging treatment multi-phase heat treatment
  • the ratio of B is in ppm by weight based on the total weight of 100 atom% in total of the composition including Ni, Al, V, Ta and Re.
  • Fig. 5 shows SEM photographs of samples No. 1 (containing Re), No. 2 (containing Re and Ta) and No. 3 (containing Ta), where for each sample, only a solution heat treatment was performed (0h), and an aging treatment (lower multi-phase heat treatment) was performed at 950°C for 2 hours (2h) and for 24 hours (24h) in addition to the solution heat treatment.
  • fine acicular particles second phase particles are precipitated at channel portions as a result of the aging heat treatment in samples No. 1 and No. 2, each of which is a Ni-based dual multi-phase intermetallic compound alloy containing Re (see 2h and 24h in No. 1 and No. 2 in Fig.
  • Vickers hardness was measured for samples No. 1 (containing Re), No. 2 (containing Re and Ta), No. 3 (containing Ta) and No. 4 (containing neither Re nor Ta: base material). Vickers hardness was measured principally with a load of 1000 g (1 kg) and a retention time of 20 seconds, and the measurement was performed at room temperature (about 25°C). The results are shown in Tables 2 and 3. Fig. 8 shows the measurement results in Table 3 in a graphical form.
  • the sample No. 4 (base material) which is a Ni-based dual multi-phase intermetallic compound alloy containing neither Re nor Ta even when an aging heat treatment is performed, Vickers hardness was little different from that when only a solution heat treatment is performed, and for the sample No. 3 (containing Ta) which is a Ni-based dual multi-phase intermetallic compound alloy containing Ta, Vickers hardness is improved as compared to the sample No. 4 (base material) due to Ta solid-solution strengthening, but Vickers hardness is only slightly increased even when the aging heat treatment is performed.
  • a Ni-based dual multi-phase intermetallic compound alloy is significantly increased in Vickers hardness when subjected to an aging heat treatment (lower multi-phase heat treatment).
  • a Ni solid solution phase is transformed into an intermetallic compound such as Ni 3 V or Ni 3 Al (regularity strengthening), and Re is precipitated as fine acicular particles (second phase particles) of a Re-rich composition (precipitation strengthening) at the channel portion of the alloy constitution, thereby causing age hardening (mechanism of age hardening by addition of Re).
  • the friction stir processing tool 1 including a Ni-based dual multi-phase intermetallic compound alloy containing Re has high hardness, has low abrasion and a long life, and can be dramatically improved in tool properties.
  • Patent Document 1 Japanese Patent Laid-open Publication No. 2009-255170
  • the friction stir processing tool 1 including a Ni-based dual multi-phase intermetallic compound alloy containing Re retains high hardness even under a high temperature.
  • Base metals of Ni, Al, V, Ta and Re (each having a purity of 99.9% by weight) and B were weighed so as to have a composition including 72 atom% of Ni, 7 atom% of Al, 13 atom% of V, 5 atom% of Ta, 3 atom% of Re and 50 ppm by weight of B, and treated by a vacuum induction melting method to prepare 0.3 kg of an ingot (cast raw material).
  • the cast raw material was cutting-processed into a tool shape shown below, and then subjected to a heat treatment at a temperature of 950°C for 5 hours as an aging heat treatment (lower multi-phase heat treatment) to prepare the present friction stir welding tool 1 shown in Fig. 1 .
  • a shoulder surface 2 is a circular flat surface having a diameter of 12 mm, and a probe 3 provided at its center is configured such that a spherical surface having a radius of 2 mm partially projects from the shoulder surface 2.
  • the diameter of the bottom part of the probe 3 is about 4 mm, the length from the shoulder surface 2 to the tip of the probe 3 (projecting height, probe length) is 0.81 mm.
  • Friction stir processing (friction stir welding by butting joint) was performed by a method shown in Fig. 2 using the friction stir processing tool 1.
  • the tool 1 was attached to a friction stir welding apparatus including three shafts: a platen shaft (X), a traverse shaft (Y) and a lifting shaft (Z).
  • a friction stir welding apparatus including three shafts: a platen shaft (X), a traverse shaft (Y) and a lifting shaft (Z).
  • an argon gas flows down along the tool side face to encompass the tool 1.
  • a platen 4 made of steel (S50C) three square poles (30 mm square, length 100 mm) made of silicon nitride, which had a smooth surface, were fixedly arranged side by side in the lengthwise direction as a backing material 5.
  • the silicon nitride as a material of the backing material 5 include, as main components, 90% by weight of Si 3 N 4 , 4 to 5% by weight of Al 2 0 3 , 4 to 5% by weight of Y 2 O 3 and so on.
  • two flat plate materials 6a and 6b made of SUS 430 (length: 300 mm, width: 75 mm and thickness: 1.0 mm) were placed and fixed on the backing material 5, with their joint surfaces butted to each other.
  • the tool 1 while rotating at a high speed of a tool rotation number of 600 to 900 rpm with a lead angle of 3 degrees, was pressed onto a joining line (butting portion 7) of two flat plate materials 6a and 6b, and after the tool 1 emitted light in orange color by frictional heat, the tool 1 rotating at a tool forwarding speed of 900 to 1400 mm/min was linearly moved to perform friction stir welding of the joining line at which two flat plate materials 6a and 6b were butted to each other.
  • the load on the tool 1 during the processing was set to 0.8 to 1.05 ton.
  • the working distance of one operation of the friction stir welding was set to 250 mm, and 80 operations were performed (total working distance: 20000 mm).
  • the friction stir welding condition was set to a fixed set value within the aforementioned conditions in one operation (friction stir welding operation with a working distance of 250 mm).
  • Figs. 9 to 15 show photographs of the joining portion of flat plate materials 6a and 6b when the number of times of the welding operation reached a predetermined number of times (see “number of times of operations" in Table 4) as test Nos. 1 to 7, and the working state of the friction stir welding was good in terms of appearance in all of initial, middle and last stages of the welding operation.
  • the tool 1 by this Example the tool 1 endured a long period of friction stir welding, and a good finishing state could be ensured over a long period of time.
  • a sample was prepared in a direction orthogonal to the joining direction, and a tensile test was conducted for examining the strength of the joining portion.
  • the sample had a width of 24.6 mm and a gauge length of 50 mm in accordance with the shape of test pieces in JIS Z No. 22015.
  • the cross head speed during measurement was 20 mm/min.
  • the result of measuring the weight of the tool 1 and the height of the probe 3 showed that after 80 times of working operations (working distance: 20000 mm) were performed, the weight of the tool 1 was decreased by 0.1 g and the height of the probe was decreased by 0.02 mm as compared to the unused state, but the tool 1 was not significantly worn away, and therefore tool abrasion was kept low.
  • the tool (tool including a Ni-based dual multi-phase intermetallic compound alloy containing Re) of Example was satisfactory in working condition in terms of appearance and joining strength even when the working distance of friction welding of a SUS 430 flat plate material reached 20000 mm, and therefore the tool life was extremely increased.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)
EP12763193.5A 2011-03-29 2012-03-27 Tool for friction stir processing and method for friction stir processing using same Not-in-force EP2692471B1 (en)

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JP2011072460A JP5998325B2 (ja) 2011-03-29 2011-03-29 摩擦攪拌加工用ツール及びこれを用いた摩擦攪拌加工方法
PCT/JP2012/057940 WO2012133412A1 (ja) 2011-03-29 2012-03-27 摩擦攪拌加工用ツール及びこれを用いた摩擦攪拌加工方法

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US9440288B2 (en) 2012-11-05 2016-09-13 Fluor Technologies Corporation FSW tool with graduated composition change
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JP6606730B2 (ja) * 2013-11-26 2019-11-20 国立大学法人大阪大学 溶接部の補強方法
JP6128671B1 (ja) * 2017-02-02 2017-05-17 ハイテン工業株式会社 熱間鍛造用金型、熱間鍛造装置、及び熱間鍛造用金型の製造方法
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EP2692471A4 (en) 2015-11-25
JPWO2012133412A1 (ja) 2014-07-28
KR20140019422A (ko) 2014-02-14
WO2012133412A1 (ja) 2012-10-04
JP2014014822A (ja) 2014-01-30
US20140027498A1 (en) 2014-01-30
US8857695B2 (en) 2014-10-14
EP2692471A1 (en) 2014-02-05
CN103492116B (zh) 2016-02-24
CN103492116A (zh) 2014-01-01
JP5998325B2 (ja) 2016-09-28

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